4-Chloro-3-[(carboxymethyl)sulfonyl]benzoic acid methyl ester → Methyl 4-chloro-3-(methylsulfonyl)benzoate
反応式
[CH3:1][O:2][C:3](=[O:18])[C:4]1[CH:9]=[CH:8][C:7]([Cl:10])=[C:6]([S:11]([CH2:14]C(O)=O)(=[O:13])=[O:12])[CH:5]=1>N1C=CC=CC=1>[CH3:1][O:2][C:3](=[O:18])[C:4]1[CH:9]=[CH:8][C:7]([Cl:10])=[C:6]([S:11]([CH3:14])(=[O:13])=[O:12])[CH:5]=1参加物
3
実験手順
4-Chloro-3-[(carboxymethyl)sulfonyl]benzoic acid methyl ester (5.6 g) was mixed with pyridine (10 mL) and the mixture was refluxed for 30 min and then cooled to room temperature. The product was precipitated by adding water (30 mL). The precipitate was filtered, washed with water and dried (yield 2.5 g). 1H-NMR (400 MHz, DMSO-d6) d=3.43 (s, 3H), 3.92 (s, 3H), 7.92 (d, J=8.2 Hz, 1H), 8.24 (dd, J=8.2 Hz, 2.2 Hz, 1H), 8.53 (d, J=2.2 Hz, 1H).
後処理
- temperaturethe mixture was refluxed for 30 min
- customThe product was precipitated
- additionby adding water (30 mL)
- filtrationThe precipitate was filtered
- washwashed with water
- customdried (yield 2.5 g)
出典と根拠
- ORDレコード
- ord-2620efac3d594871b2efc815fec98769
- 出典データセット
- uspto-grants-2001_03
- 特許番号
- US06201027B1
反応ノート
読み込み中…